CN115606606A - Novel metal polyphenol network loaded metal oxide antibacterial nanoparticles, preparation method and application - Google Patents
Novel metal polyphenol network loaded metal oxide antibacterial nanoparticles, preparation method and application Download PDFInfo
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- CN115606606A CN115606606A CN202211223610.9A CN202211223610A CN115606606A CN 115606606 A CN115606606 A CN 115606606A CN 202211223610 A CN202211223610 A CN 202211223610A CN 115606606 A CN115606606 A CN 115606606A
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- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 77
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 62
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 56
- 239000002184 metal Substances 0.000 title claims abstract description 56
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 60
- 229910021645 metal ion Inorganic materials 0.000 claims description 39
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- 239000001648 tannin Substances 0.000 claims description 18
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 17
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- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 7
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 6
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- 229910021550 Vanadium Chloride Inorganic materials 0.000 claims description 6
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- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 claims description 4
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- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 claims description 4
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
- A01N55/02—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur containing metal atoms
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
- A61L2/088—Radiation using a photocatalyst or photosensitiser
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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Abstract
The invention provides a novel metal polyphenol network loaded metal oxide antibacterial nano particle and a preparation method thereof, wherein a uniformly dispersed and stable metal-polyphenol complex network is prepared by taking a large amount of phenolic hydroxyl groups carried by polyphenol as active sites through a one-step blending method, and the antibacterial nano particle with high stability and high photothermal conversion capability is obtained on the basis of no help of a traditional photosensitizer/photothermal agent by utilizing the sensitization effect of the network on the metal oxide and the excellent photothermal conversion capability and naturalness of the network.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to novel metal polyphenol network loaded metal oxide antibacterial nanoparticles, a preparation method and application.
Background
The traditional antibacterial strategy is to use antibacterial materials containing antibiotics, but the wide use of antibiotics causes the bacteria to generate drug resistance, thereby increasing the cost and difficulty of resisting bacterial pollution. Therefore, in recent years, research in the antibacterial field has been devoted to preventing the development of bacterial resistance and to exploring broad-spectrum antibacterial strategies.
The photodynamic antibacterial strategy and the photothermal antibacterial strategy are novel non-antibiotic antibacterial strategies which do not cause the generation of bacterial drug resistance.
The photodynamic therapy utilizes photosensitizer which can generate active oxygen under an excitation light source with proper wavelength to generate oxidative damage to surrounding biological molecules such as lipid, protein, nucleic acid and the like, thereby killing cancer cells or pathogenic microorganisms; photothermal therapy converts the energy of near infrared light into heat energy using a photothermal agent, thereby destroying bacteria using the heat energy. Compared with the traditional non-photodynamic free radical activation antibacterial therapy, the photodynamic antibacterial therapy has the following advantages: 1) By means of the light source, the antibacterial treatment is more targeted (local treatment); 2) No restriction of hydrogen peroxide concentration in the microenvironment of the infected site; 3) The active oxygen is rich in types.
The synergistic effect generated by the combination of the photothermal antibacterial therapy and the photodynamic antibacterial therapy can improve the antibacterial specificity and the treatment effect and reduce the damage of normal cells and tissues caused by overhigh temperature.
However, as far as now is concerned, on the one hand, conventional photosensitizers/photothermals may have some impact on the environment; on the other hand, the conventional photosensitizer/photothermal agent needs to reach a certain content to achieve the ideal photodynamic/photothermal effect for biofilm ablation, but too high dosage may cause aggregation of the photosensitizer/photothermal agent to affect the photothermal conversion rate, and may cause harm to healthy cells, thereby limiting the application of the photosensitizer/photothermal agent in antibacterial aspect.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a novel metal polyphenol network loaded metal oxide antibacterial nano particle and a preparation method thereof, wherein a uniformly dispersed and stable metal-polyphenol complex network wrapped with metal oxide is prepared by a one-step blending method, the metal-polyphenol complex network not only can enhance the utilization rate of a metal oxide semiconductor to visible light, but also can convert light energy into heat energy, can locally heat while online generating active oxygen ROS, and can generate oxygen toxicity and thermal ablation on bacterial cells without adding any photosensitizer and photo-thermal agent, thereby achieving the antibacterial effect.
According to a first aspect of the present invention, there is provided a novel metal polyphenol network loaded metal oxide antibacterial nanoparticle, the nanoparticle comprising a metal-polyphenol complex network formed by coordination of metal ions and polyphenols, the metal-polyphenol complex network being encapsulated with a metal oxide;
wherein the metal ions are metal ions having absorption in the near infrared and/or metal ions capable of d-d transition;
the metal oxide is a nano semiconductor metal oxide.
Preferably, when only near-infrared illumination is selected, metal ions that absorb in the near-infrared are employed.
Preferably, when only solar irradiation is selected, metal ions capable of d-d transition are used.
Preferably, when the irradiation of both sunlight and near infrared light is selected, metal ions satisfying both absorption in the near infrared and d-d transition are used.
According to the second aspect of the present invention, there is provided a method for preparing the novel metal polyphenol network-supported metal oxide antibacterial nanoparticles, comprising the following steps:
respectively dissolving polyphenol and metal salt in deionized water to obtain polyphenol aqueous solution and metal precursor salt solution; wherein, the metal ions in the metal salt are metal ions which have absorption in near infrared and/or metal ions which can generate d-d transition;
dissolving a metal oxide in a Tris-HCl buffer solution to obtain a first solution; wherein the metal oxide is a nano semiconductor metal oxide;
adding the polyphenol aqueous solution and the metal precursor salt solution into the first solution at the same time, stirring and adjusting the pH value to be more than or equal to 7 to obtain a second solution;
and centrifuging the second solution, washing, vacuum-drying, crushing and grinding the centrifuged product to obtain the novel metal polyphenol network-loaded metal oxide antibacterial nanoparticles.
Preferably, the metal salt is ferric chloride hexahydrate, copper chloride dihydrate, zinc chloride, vanadium chloride or ruthenium chloride.
Preferably, the metal oxide is nano titanium dioxide, nano zinc oxide, nano copper oxide or nano molybdenum dioxide.
Preferably, the polyphenol is epigallocatechin gallate, cercis negundo tannin or tannic acid.
Preferably, the mass concentration ratio of the metal ions in the polyphenol water solution and the metal precursor salt solution is 1 (1-4).
Preferably, the mass ratio of the metal oxide to the Tris-HCl buffer solution in the first solution is 1 (1-2), and the pH value of the Tris-HCl buffer solution is 7-8.
Preferably, the polyphenol aqueous solution and the metal precursor salt solution are simultaneously added into the first solution, stirred and adjusted to pH 7-8 to obtain a second solution.
According to the third aspect of the invention, the application of the metal oxide antibacterial nanoparticles loaded on the novel metal polyphenol network in preparing antibacterial materials is provided.
According to the technical scheme, the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles provided by the invention have the advantages that under the irradiation of near infrared light, after the polyphenol-metal complex network absorbs light energy, metal ions in the network form electrons and holes, the electron energy is released in a non-radiation attenuation channel, lattice vibration is caused to generate abundant phonons and lattice heat, heat is generated, a photo-thermal platform is formed, protein and collagen are denatured, cell membrane permeability is realized, and the toxic and side effects of a photo-thermal agent in the synthesis and use processes are effectively solved.
Meanwhile, the polyphenol-metal complex network can transmit absorbed light energy to the nano semiconductor, so that the band gap of the nano semiconductor is narrowed, the potential of a conduction band is more negative, and the reduction of oxygen adsorbed on the surface into O is facilitated 2 · — And further becomes singlet oxygen, and the singlet oxygen is utilized to damage proteins, fat and other biomolecules around the photosensitization position, so that cells are killed, the problems of aggregation, limited absorption and the like of a photosensitizer are effectively solved, and the problem that normal and healthy cells are accidentally injured due to overhigh temperature in photothermal therapy is avoided.
Therefore, the photodynamic force and the photothermal force have synergistic effect, so that the energy can be dispersed to the photodynamic force for antibacterial action, and the overhigh temperature of photothermal treatment is avoided; also can utilize the polyphenol metal network with higher photo-thermal conversion efficiency to achieve a certain antibacterial effect.
The novel metal polyphenol network loaded metal oxide antibacterial nano particles can meet the requirement of antibiosis under sunlight by adjusting the types of metal ions, and the polyphenol-metal complex network absorbs the sunlight, on one hand, partial energy is transferred to the nano metal oxide semiconductor, so that the band gap of the nano metal oxide semiconductor is narrowed, the conduction band potential is more negative, and the reduction of oxygen adsorbed on the surface to O is more facilitated 2 · — Further becomes singlet oxygen; on the other hand, the other part of energy for absorbing sunlight is transferred to the unoccupied d orbitals in the metal ions to generate internal d-d transition, so that the band gap of the polyphenol is reduced, and the light absorption capacity and the total photothermal effect of the obtained polyphenol material are further improved.
Drawings
Fig. 1 is a schematic structural diagram of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles of the present invention.
Fig. 2 is a picture of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles of the present invention after redissolution.
Fig. 3 is a picture of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles of the present invention after redissolution.
FIG. 4 is a graph showing the antibacterial property test of the nanoparticles obtained in example 1 of the present invention and the material obtained in the comparative example.
Detailed Description
In order to better understand the technical content of the present invention, specific embodiments are described below with reference to the accompanying drawings.
In this disclosure, aspects of the present invention are described with reference to the accompanying drawings, in which a number of illustrative embodiments are shown. Embodiments of the present disclosure are not necessarily intended to encompass all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in greater detail below, may be implemented in any of numerous ways.
The principle of photodynamic therapy is as follows: under the irradiation of a light source with the wavelength consistent with the absorption wavelength of photosensitizer molecules, the photosensitizer absorbs electrons and is converted from a singlet state ground state to a singlet excited state; part of the energy is radiated as a fluorescence quantum, and the rest of the energy transforms the photosensitizer molecule into a triplet state (a therapeutically useful form), which is transferred to a ground state oxygen molecule, which transforms the oxygen molecule from the ground state to an excited state to generate singlet oxygen.
The principle of the photothermal therapy is as follows: under the irradiation of near infrared light (700-1100 nm), the photothermal reagent is converted into an excited state to form electrons and holes, the energy of the electrons is released in a non-radiative decay channel (the lattice vibration can be caused to emit abundant phonons and lattice heat), and heat is generated to denature proteins and collagen and realize cell membrane permeability.
In the traditional photodynamic therapy, a photosensitizer is needed, the photosensitizer is easy to gather due to the use of a large amount of the photosensitizer, the curative effect of the traditional photodynamic therapy is influenced due to limited penetration of laser to deep tissues and limited absorption of laser by the photosensitizer, and the environment is influenced due to the use of a large amount of the photosensitizer.
The traditional photothermal agent has a complex synthesis process, needs complex chemicals and toxic additives, is not environment-friendly, is easy to aggregate due to the use of a large amount of photothermal agent, influences the curative effect, and causes overhigh temperature due to the large amount of heat generated by the photothermal agent, thereby damaging normal cells and tissues.
Therefore, the invention provides a novel metal polyphenol network loaded metal oxide antibacterial nano particle and a preparation method thereof, wherein a uniformly dispersed and stable metal-polyphenol complex network is prepared by a one-step blending method by taking a large number of phenolic hydroxyl groups carried by polyphenol as active sites, and the antibacterial nano particle with high stability and high photothermal conversion capability is obtained by utilizing the sensitization effect of the network on the metal oxide and the excellent photothermal conversion capability and naturalness of the network on the basis of not depending on the traditional photosensitizer/photothermal agent.
In an exemplary embodiment of the present invention, a novel metal polyphenol network loaded metal oxide antibacterial nanoparticle is provided, the nanoparticle comprising a metal-polyphenol complex network formed by coordination of metal ions and polyphenols, wherein the metal oxide is encapsulated in the metal-polyphenol complex network.
Wherein the metal ions are metal ions having absorption in the near infrared and/or metal ions capable of d-d transition.
The metal oxide is a nano semiconductor metal oxide.
As shown in figure 1, the metal ions and polyphenol are coordinated to form a metal-polyphenol complex network, and the metal-polyphenol complex network is coated on the surface of the metal oxide, because the network is compact and uniform, the metal oxide can be coated in multiple directions, and the metal oxide is wrapped.
In one preferred embodiment, when only near-infrared illumination is selected, metal ions that absorb in the near-infrared are employed, e.g., ferric ions, gold ions, vanadium ions, ruthenium ions, and the like.
In one preferred embodiment, when only solar irradiation is selected, metal ions that can undergo d-d transition are used, for example, transition metal ions, ferric ions, gold ions, vanadium ions, ruthenium ions, copper ions, zinc ions, and the like.
In one preferred embodiment, when the irradiation is performed by using either sunlight or near infrared light, metal ions which have both absorption in the near infrared and d-d transition can be used, such as ferric ions, gold ions, vanadium ions, ruthenium ions, zinc ions, etc.
The invention also provides a preparation method of the novel metal polyphenol network loaded metal oxide antibacterial nano particles, a large number of phenolic hydroxyl groups carried by polyphenol can be complexed with metal ions through a one-step blending method, stable coordination property can be shown on the surface of metal oxide, materials can be formed in water within a few minutes, additional conditions and additives are not needed, the preparation cost is low, and the preparation method is green and environment-friendly.
In another exemplary embodiment of the present invention, there is provided a method for preparing the novel metal polyphenol network-supported metal oxide antibacterial nanoparticles, comprising the following steps:
respectively dissolving polyphenol and metal salt in deionized water to obtain polyphenol aqueous solution and metal precursor salt solution; wherein the metal ions in the metal salt are metal ions having absorption in the near infrared and/or metal ions capable of d-d transition.
Dissolving a metal oxide in a Tris-HCl buffer solution to obtain a first solution; wherein the metal oxide is a nano semiconductor metal oxide.
And simultaneously adding the polyphenol aqueous solution and the metal precursor salt solution into the first solution, stirring and adjusting the pH value to be more than or equal to 7 to obtain a second solution.
And centrifuging the second solution, washing, vacuum-drying, crushing and grinding the centrifuged product to obtain the novel metal polyphenol network-loaded metal oxide antibacterial nanoparticles.
In a preferred embodiment, the metal salt is ferric chloride hexahydrate, cupric chloride dihydrate, zinc chloride, vanadium chloride or ruthenium chloride.
In a preferred embodiment, the metal oxide is nano titanium dioxide, nano zinc oxide, nano copper oxide or nano molybdenum dioxide.
In preferred embodiments, the polyphenol is epigallocatechin gallate (EGCG), acacia negra tannin (OPC), or Tannic Acid (TA).
In a preferred embodiment, the mass concentration ratio of the metal ions in the polyphenol water solution and the metal precursor salt solution is 1 (1-4).
In a preferred embodiment, the mass ratio of the metal oxide to the Tris-HCl buffer solution in the first solution is 1 (1-2), and the pH value of the Tris-HCl buffer solution is 7-8.
In a preferred embodiment, the polyphenol aqueous solution and the metal precursor salt solution are added simultaneously to the first solution, stirred and adjusted to pH 7-8 to obtain a second solution.
The deprotonation degree of the hydroxyl group is controlled by using pH, and the protonation is enhanced by using a single complex when the pH is less than or equal to 2; the double complex compound is formed when the pH value is 3-6; when the pH value is more than or equal to 7, the ternary complex is formed, and protonation is the weakest.
The selection of the proper pH condition can inhibit the protonation of the phenolic hydroxyl group and play the role of the phenolic hydroxyl group.
In another exemplary embodiment of the present invention, there is also provided a use of the metal oxide antibacterial nanoparticles loaded on the novel metal polyphenol network in preparation of an antibacterial material.
As shown in fig. 2 and 3, the nanoparticle is a solution having a certain viscosity after being redissolved (as can be seen from fig. 2 and 3, the solution has a certain wall-hanging property, which can be explained as having a certain viscosity), and therefore, the following applications can be made:
(1) the antibacterial film is formed on the medical appliance by spraying, reduces the adhesion of bacteria and prolongs the service life of the appliance
(2) Spraying on clothes, insole, bed sheet, quilt cover, and fruit for inhibiting bacteria
(3) The coating is coated on the outermost layer of glasses, goggles, masks and the like through simple dip coating to inhibit bacteria
(4) Surface modified nanofiltration membrane for preventing biofilm contamination and bacterial infection
(5) The hydrogel can be used as wound dressing or for purifying sewage and simultaneously improving bacterial contamination
The application of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles in preparing antibacterial materials includes but is not limited to the application scenes.
For better understanding, the present invention is further described below with reference to several specific examples, but the materials and processing techniques are not limited thereto, and the present disclosure is not limited thereto.
Example 1
Step one, respectively dissolving 0.2g of black wattle tannin and 0.242g of ferric trichloride hexahydrate in 50mL of deionized water at room temperature to obtain 4mg/mL of tannin aqueous solution and 1mg/mL of ferric trichloride aqueous solution.
And step two, dissolving 100mg of nano titanium dioxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three, centrifuging for 10min at the rotating speed of 8000rpm, washing for 3 times by using deionized water respectively, then carrying out vacuum drying at 60 ℃, and crushing and grinding to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 2
Step one, respectively dissolving 0.2g of black wattle tannin and 0.484g of ferric trichloride hexahydrate in 50mL of deionized water at room temperature to obtain 4mg/mL of tannin aqueous solution and 2mg/mL of ferric trichloride aqueous solution.
And step two, dissolving 100mg of nano zinc oxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 8 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three at a rotating speed of 9000rpm for 10min, washing with deionized water for 3 times respectively, then carrying out vacuum drying at 80 ℃, and crushing and grinding to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 3
Step one, respectively dissolving 0.2g of tannic acid and 0.968g of ferric trichloride hexahydrate in 50mL of deionized water at room temperature to obtain 4mg/mL of tannic acid aqueous solution and 4mg/mL of ferric trichloride aqueous solution.
And step two, dissolving 100mg of nano titanium dioxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three at the rotating speed of 10000rpm for 5min, washing the solution with deionized water for 3 times respectively, then drying the solution in vacuum at 70 ℃, and crushing and grinding the dried solution to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 4
Step one, respectively dissolving 0.2g of cercis negundo tannin and 0.968g of vanadium chloride in 50mL of deionized water at room temperature to obtain a tannin aqueous solution of 4mg/mL and a vanadium chloride aqueous solution of 4 mg/mL.
And step two, dissolving 100mg of nano molybdenum dioxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three, centrifuging for 5min at the rotating speed of 10000rpm, washing for 3 times by using deionized water respectively, then drying in vacuum at 70 ℃, and crushing and grinding to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 5
Step one, respectively dissolving 0.2g of black wattle tannin and 0.968g of ruthenium chloride in 50mL of deionized water at room temperature to obtain 4mg/mL of tannin aqueous solution and 4mg/mL of ruthenium chloride aqueous solution.
And step two, dissolving 100mg of nano titanium dioxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three, centrifuging for 5min at the rotating speed of 10000rpm, washing for 3 times by using deionized water respectively, then drying in vacuum at 70 ℃, and crushing and grinding to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 6
Step one, respectively dissolving 0.2g of cercis negundo tannin and 0.968g of copper chloride dihydrate into 50mL of deionized water at room temperature to obtain 4mg/mL tannin aqueous solution and 4mg/mL vanadium chloride aqueous solution.
And step two, dissolving 100mg of nano copper oxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three at the rotating speed of 10000rpm for 5min, washing the solution with deionized water for 3 times respectively, then drying the solution in vacuum at 70 ℃, and crushing and grinding the dried solution to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Example 7
Step one, respectively dissolving 0.2g of black wattle tannin and 0.968g of zinc chloride in 50mL of deionized water at room temperature to obtain a 4mg/mL tannin aqueous solution and a 4mg/mL ruthenium chloride aqueous solution.
And step two, dissolving 100mg of nano titanium dioxide powder in 50mL of Tris-HCl buffer solution with the pH value of 8.
And step three, simultaneously adding the aqueous solution obtained in the step one into the solution obtained in the step two, stirring and adjusting the pH to 7 by using 0.1M sodium hydroxide solution.
And step four, centrifuging the solution obtained in the step three, centrifuging for 5min at the rotating speed of 10000rpm, washing for 3 times by using deionized water respectively, then drying in vacuum at 70 ℃, and crushing and grinding to obtain the novel metal-polyphenol network loaded metal oxide antibacterial particles.
Comparative example
Step one, respectively dissolving 0.2g of black wattle tannin and 0.242g of ferric trichloride hexahydrate in 50mL of deionized water at room temperature to obtain 4mg/mL of tannin aqueous solution and 1mg/mL of ferric trichloride aqueous solution.
And step two, simultaneously adding the aqueous solution obtained in the step one into a Tris-HCl buffer solution with the pH value of 8, stirring and adjusting the pH value to 7 by using a 0.1M sodium hydroxide solution.
And step three, centrifuging the solution obtained in the step two for 10min at the rotating speed of 8000rpm, washing the solution for 3 times respectively by using deionized water, then carrying out vacuum drying at the temperature of 60 ℃, and crushing and grinding the solution to obtain a control group experiment sample.
Antibacterial testing
Using the nanoparticles (FOT) obtained in example 1, the material (FO) obtained in comparative example, and TiO 2 An antibacterial test was performed and a pure bacterial solution (E.coli) was used as a blank control.
Near infrared light (700-1100 nm)
The experimental steps are as follows: preparing a sample bacterial suspension mixture with the sample concentration of 5mg/mL, specifically a mixture formed by the bacterial suspension of the sample and escherichia coli in sterile PBS, culturing in an incubator at 37 ℃ for 0.5h, and illuminating for 10min under a near-infrared light source.
The mixture was then diluted with a sterile 1X PBS solution gradient, 100 μ L of the above mixture solution was placed in a petri dish with solid medium and bacterial plating was performed using a spreading rod. And (3) after the culture dish after being plated is placed in an incubator at 37 ℃ for culturing for 16-24h, observing the colony number on the surface of the solid culture medium, and photographing and recording.
Under the condition of simulating sunlight
The experimental steps are as follows: preparing a sample bacterial suspension mixture with the sample concentration of 5mg/mL, specifically a mixture formed by the bacterial suspension of the sample and escherichia coli in sterile PBS, culturing in an incubator at 37 ℃ for 0.5h, and illuminating for 30min under a 300W xenon lamp simulated sunlight source. The mixture was then diluted with sterile 1X PBS gradient, 100 μ L of the above mixture solution was placed in a petri dish with solid medium and bacterial plating was performed using a spreading rod. And (3) after the culture dish after being plated is placed in an incubator at 37 ℃ for culturing for 16-24h, observing the colony number on the surface of the solid culture medium, and photographing and recording.
As shown in fig. 4, tables 1 and 2, it can be seen from fig. 4, tables 1 and 2 that the antibacterial effect of the material with metal oxide added is better than that without the metal oxide added under the near infrared light condition and the solar light condition, and the antibacterial efficiency can reach more than 95% under the near infrared condition and 90% under the sunlight, which indicates that the antibacterial particles of the present invention can absorb the near infrared light to achieve the antibacterial effect, and can achieve better antibacterial performance by the "sensitization" of the tannin metal complex network and the d-d transition of the metal ions.
TABLE 1 antimicrobial testing in the near Infrared
Table 2 antimicrobial testing under simulated sunlight
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (12)
1. A novel metal polyphenol network loaded metal oxide antibacterial nano particle is characterized in that the nano particle comprises a metal-polyphenol complex network formed by coordination of metal ions and polyphenol, wherein the metal oxide is wrapped in the metal-polyphenol complex network;
wherein the metal ions are metal ions having absorption in the near infrared and/or metal ions capable of generating d-d transition;
the metal oxide is a nano semiconductor metal oxide.
2. The novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 1, wherein when only near infrared irradiation is selected, metal ions having absorption in the near infrared are used.
3. The novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 1, wherein when only sunlight irradiation is selected, metal ions capable of d-d transition are used.
4. The novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 1, wherein when the nanoparticles are irradiated by sunlight or near infrared light, metal ions which have absorption in the near infrared and can perform d-d transition are used.
5. A method for preparing novel metal polyphenol network loaded metal oxide antibacterial nanoparticles as claimed in any one of claims 1-4, which is characterized by comprising the following steps:
respectively dissolving polyphenol and metal salt in deionized water to obtain polyphenol aqueous solution and metal precursor salt solution; wherein, the metal ions in the metal salt are metal ions which can absorb in near infrared and/or metal ions which can generate d-d transition;
dissolving a metal oxide in a Tris-HCl buffer solution to obtain a first solution; wherein the metal oxide is a nano semiconductor metal oxide;
adding the polyphenol aqueous solution and the metal precursor salt solution into the first solution at the same time, stirring and adjusting the pH value to be more than or equal to 7 to obtain a second solution;
and centrifuging the second solution, washing, vacuum drying, crushing and grinding the centrifuged product to obtain the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles.
6. The method for preparing novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 5, wherein the metal salt is ferric chloride hexahydrate, cupric chloride dihydrate, zinc chloride, vanadium chloride or ruthenium chloride.
7. The preparation method of the novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 5, wherein the metal oxide is nano titanium dioxide, nano zinc oxide, nano copper oxide or nano molybdenum dioxide.
8. The method for preparing novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 5, wherein the polyphenol is epigallocatechin gallate, cercis tannin or tannic acid.
9. The preparation method of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles as claimed in claim 5, wherein the mass concentration ratio of metal ions in the polyphenol aqueous solution and the metal precursor salt solution is 1 (1-4).
10. The preparation method of the novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 5, wherein the mass ratio of the metal oxide to the Tris-HCl buffer solution in the first solution is 1 (1-2), and the pH value of the Tris-HCl buffer solution is 7-8.
11. The method for preparing novel metal polyphenol network-supported metal oxide antibacterial nanoparticles as claimed in claim 5, characterized in that the polyphenol aqueous solution and the metal precursor salt solution are added into the first solution at the same time, stirred and adjusted to pH 7-8 to obtain the second solution.
12. Use of the novel metal polyphenol network loaded metal oxide antibacterial nanoparticles as defined in any one of claims 1 to 4 in the preparation of antibacterial materials.
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